High-purity ozone concentration process and device for cleaning and etching of semiconductor materials

Abstract

The present application relates to the technical field of ozone compression, and in particular to a high-purity ozone concentration process and device for cleaning and etching of semiconductor materials, which includes the following steps: gas compression: compressing the gas to form a pressurized initial gas; adsorption separation: passing the pressurized initial gas into the ozone concentration device, and balancing the concentration of the pressurized initial gas, setting two layers of adsorbent to jointly adsorb ozone, and during adsorption, adjusting the relative positions of the two layers of adsorbent, changing the gas flushing position, and forming a combination of fixed adsorption and flow adsorption; desorption: separating ozone and compressing to form high-purity ozone concentrated gas; wherein the device includes: a tower body, an adsorbent layer, an air inlet pipe for gas supply, an exhaust pipe for exhaust, a sealing plate sliding in the air inlet pipe for adjusting the air supply of the air inlet pipe, a sliding mechanism for driving the sealing plate to slide, and an exhaust module for separating and desorbing ozone. The present application has the effect of reducing the impact on the purity of the ozone concentrated gas.

Description

Technical Field

[0001] The present application relates to the technical field of ozone compression, and in particular to a high-purity ozone concentration process and device for cleaning and etching semiconductor materials. Background Art

[0002] At present, with the rapid development of semiconductor technology, chip process nodes are constantly shrinking, and the requirements for the cleanliness and process precision of the semiconductor material surface are getting higher and higher. In the semiconductor manufacturing process, cleaning and etching are key process steps, which directly affect the performance and yield of the chip; ozone, as an efficient oxidant, has been widely used in the cleaning and etching links in semiconductor manufacturing due to its strong oxidizing properties.

[0003] In the prior art, ozone is concentrated, generally using an ozone generator to produce ozone, and then passing through an adsorption tower to separate ozone from other gas components, and then separating the ozone in the adsorption tower to form high-purity concentrated ozone, which is then used as an oxidant for cleaning and etching semiconductor materials. However, when the adsorption tower is performing ozone adsorption, ozone is generally supplied from the bottom of the adsorption tower, and the ozone first contacts with the adsorbent at the lower end, which will first perform adsorption. As the gas rises, the adsorbable components gradually decrease, and the lower adsorbent is saturated earlier than the upper adsorbent, resulting in the adsorption efficiency of the lower adsorbent being reduced or returning to zero during continuous ventilation, which affects the purity and recovery efficiency of the ozone concentrated gas. Summary of the invention

[0004] In order to reduce the impact on the purity of ozone concentrated gas, the present application provides a high-purity ozone concentration process and device for use in cleaning and etching of semiconductor materials.

[0005] In the first aspect, the present application provides a high-purity ozone concentration process for cleaning and etching semiconductor materials, which adopts the following technical solution:

[0006] A high-purity ozone concentration process for cleaning and etching semiconductor materials comprises the following steps:

[0007] Gas compression: The mixed gas of ozone and oxygen is pressurized after dehydration to form a pressurized initial gas;

[0008] Adsorption separation: The pressurized initial gas is introduced into the ozone concentrator, and when the pressurized initial gas is introduced into the ozone concentrator, the gas supply position of the pressurized initial gas is adjusted so that the concentration of the pressurized initial gas in the ozone concentrator is balanced and contacts with the adsorbent in the ozone concentrator; two layers of adsorbent are provided to jointly adsorb ozone, and during adsorption, an adjustment module is provided to adjust the relative positions of the two layers of adsorbent, change the flushing position of the gas, and form a combination of fixed adsorption and flow adsorption;

[0009] Desorption: The ozone adsorbed by the adsorbent is separated from the adsorbent by vacuuming, and then compressed to form high-purity ozone concentrated gas.

[0010] By adopting the above technical scheme, the mixed gas of ozone and oxygen is dehydrated and pressurized through the gas compression step, which helps to reduce the moisture and other impurities in the gas and provide a relatively pure initial gas for the subsequent steps; in the adsorption separation step, by adjusting the gas supply position of the pressurized initial gas and adopting a combination of fixed adsorption and flow adsorption, the adsorption capacity of the adsorbent can be more effectively utilized to achieve efficient separation and enrichment of ozone, thereby improving the concentration and purity of the finally obtained ozone concentrated gas; adjusting the gas supply position to make the concentration of the pressurized initial gas in the ozone concentrator balanced can avoid the adsorption caused by excessively high or low local concentrations The adsorption efficiency decreases, ensuring that the adsorbent can fully utilize its adsorption capacity; the combination of fixed adsorption and flow adsorption can dynamically adjust the use status of the adsorbent, avoiding the problem of too fast adsorbent saturation or insufficient utilization that may be caused by a single adsorption method, thereby improving the overall adsorption efficiency; the use of vacuum desorption can significantly reduce the pressure on the adsorbent surface, making it easier for the adsorbed ozone to desorb from the adsorbent, thereby improving the desorption efficiency and ozone recovery rate; the desorbed ozone can be further concentrated and purified after compression treatment, providing a high-quality, high-concentration ozone source for applications such as semiconductor material cleaning and etching.

[0011] Optionally, in the adsorption separation step, when adjusting the supply position of the pressurized initial gas, an intermittent gas supply from bottom to top is adopted to adjust the concentration of the pressurized initial gas inside the ozone concentrator.

[0012] By adopting the above technical scheme, the bottom-up gas supply method can ensure that the gas distribution in the ozone concentration device is more uniform. Since the gas enters from the bottom, it will gradually rise and fully contact with the adsorbent. By adjusting the upper and lower intermittent gas supply, it is easy to adjust the concentration of the absorbable gas in the upper part, thereby reducing the possibility of local concentration being too high or too low; this method helps to avoid the decrease in adsorption efficiency caused by excessive concentration gradient, so that the adsorbent can more effectively utilize its adsorption capacity and improve the adsorption efficiency of ozone; through reasonable intermittent time setting, it can be ensured that the adsorbent is in the best working state every time the gas is supplied, thereby improving its utilization efficiency and service life; the bottom-up intermittent gas supply method helps to reduce fluctuations and uncertainties in the process; since the gas distribution is more uniform and the adsorption efficiency is more stable, the stability of the entire process will also be improved.

[0013] Optionally, in the adsorption separation step, when the pressurized initial gas is supplied, the pressurized initial gas is pumped and agitated.

[0014] By adopting the above technical solution, whipping and stirring can increase the turbulence of the gas and whip the entry position of the pressurized initial gas, thereby promoting more complete mixing and dispersion of ozone and oxygen in the pressurized initial gas, which helps to reduce the concentration gradient of the gas itself, allowing the adsorbent to more evenly contact the ozone in the pressurized initial gas and improve the adsorption efficiency.

[0015] Beating and agitation can increase the movement speed and kinetic energy of gas molecules, thereby promoting the diffusion and adsorption of gas molecules on the adsorbent surface; this helps to improve the adsorption rate and adsorption capacity, making the adsorption process more efficient and faster; beating and agitation can make the gas distribution in the adsorption bed more uniform, avoid local blockage or gas short-circuiting and other problems, and at the same time, enable the pressurized initial gas to obtain initial irregular kinetic energy. It can also promote the relative movement between adsorbent particles, prevent particle agglomeration and compaction, thereby maintaining the good structure and permeability of the adsorption bed.

[0016] In the second aspect, the present application provides a high-purity ozone concentration device for cleaning and etching semiconductor materials, which adopts the following technical solution:

[0017] A high-purity ozone concentration device used for cleaning and etching of semiconductor materials, comprising:

[0018] The tower body has a reaction chamber formed therein;

[0019] An adsorbent layer is arranged in the tower body, annularly arranged around the central axis of the tower body, and divides the reaction chamber into an adsorption chamber and a miscellaneous gas chamber;

[0020] An air inlet pipe is arranged on the tower body, extends from the bottom to the top of the tower body, is located in the adsorption chamber, and is provided with a plurality of air inlet holes communicating with the adsorption chamber;

[0021] An exhaust pipe, arranged on the tower body and connected to the impurity chamber, is used to discharge the remaining gas after the adsorption is completed;

[0022] A sealing plate is slidably mounted in the air inlet pipe and is provided with a plurality of communication holes in the vertical direction. The communication holes correspond to and are connected with the air inlet holes. In an initial state, the air inlet holes at the lower end are misaligned and blocked with the communication holes. As the sealing plate slides, the air inlet holes at the lower end are opened.

[0023] A sliding mechanism, arranged on the air inlet pipe and connected to the sealing plate, and used for driving the sealing plate to slide;

[0024] The exhaust module is communicated with the adsorption chamber and is used to extract the ozone adsorbed by the adsorbent layer and compress it.

[0025] By adopting the above technical solution, when the device is in a non-working state, the sealing plate is located at the initial position in the air inlet pipe. At this time, the air inlet hole at the lower end and the connecting hole on the sealing plate are offset and blocked to prevent the pressurized initial gas (a mixture of ozone and oxygen) from directly entering the adsorption chamber; when it is necessary to start working, the pressurized initial gas first rises in the air inlet pipe until it fills the air inlet pipe, and the sliding mechanism is started to drive the sealing plate to slide upward in the vertical direction. As the sealing plate moves, the air inlet hole at the lower end gradually aligns with and connects with the connecting hole, allowing the pressurized initial gas to enter the adsorption chamber through the air inlet hole and the connecting hole, so that the air inlet pipe supplies air to the air inlet chamber at the same time from top to bottom.

[0026] The pressurized initial gas entering the adsorption chamber contacts the adsorbent layer, and the ozone is adsorbed by the adsorbent, while the unabsorbed gas (mainly oxygen) enters the mixed gas chamber and is then discharged through the exhaust pipe.

[0027] As the sealing plate continues to slide, more air inlet holes are connected to the connecting holes, allowing more pressurized initial gas to enter the adsorption chamber. At the same time, due to the sliding of the sealing plate, the amount of gas entering the adsorption chamber can be gradually adjusted to achieve precise control of the adsorption process, and the gas can be controlled to keep the concentration of the pressurized initial gas consistent when entering the adsorption chamber, so that the gas concentration in the air inlet pipe tends to be consistent, thereby making the effect of adjusting the concentration easier to adsorb the adsorbent and reducing the situation where the lower adsorbent is saturated before the upper adsorbent, so that in the process of continuous ventilation, the adsorption efficiency of the lower adsorbent is consistent with that of the upper adsorbent, so that the purity and recovery efficiency of the ozone concentrated gas can be maintained.

[0028] When the adsorbent layer reaches a certain adsorption saturation, the exhaust module is started. The exhaust module is connected to the adsorption chamber to extract the ozone adsorbed on the adsorbent layer and compress it to form high-purity ozone concentrated gas. The compressed high-purity ozone concentrated gas is discharged through the exhaust module for use in subsequent semiconductor material cleaning, etching and other processes.

[0029] Optionally, the sliding mechanism comprises:

[0030] A rotating ring is rotatably disposed in the air inlet pipe and abuts against one end of the sealing plate close to the bottom wall of the tower body;

[0031] A first protrusion is provided on the rotating ring, faces the sealing plate, and abuts against the sealing plate;

[0032] A second protrusion, disposed on the sealing plate, abutting against the first protrusion or the rotating ring;

[0033] The power assembly is arranged in the air inlet pipe and connected with the rotating ring to drive the rotating ring to rotate.

[0034] By adopting the above technical solution, the rotating ring is rotatably arranged in the air inlet pipe and abuts against one end of the sealing plate close to the bottom wall of the tower body. The sealing plate is provided with a first protrusion, which faces the rotating ring and abuts against a certain part of the rotating ring; the rotating ring is also provided with a second protrusion, which may directly abut against the first protrusion, or abut against other parts of the sealing plate in some cases; the power assembly has been installed and connected to the rotating ring, ready to provide rotational power; when the position of the sealing plate or the rotating ring needs to be adjusted, the power assembly is started, the power assembly starts to work, and drives the rotating ring to rotate, and as the rotating ring With the rotation of the second protrusion, the second protrusion moves relative to the first protrusion or other parts of the sealing plate, so that the first protrusion and the second protrusion reciprocate to abut and separate, so that the sealing plate slides up and down by relying on its own gravity and the abutting force of the protrusions, thereby adjusting the position of the sealing plate, and then realizing the cyclic blocking and opening of the air inlet hole at the lower end of the air inlet pipe; realizing automatic adjustment in the process of air supply, thereby improving the automation level of the equipment, and the automatic adjustment method makes the upper and lower concentrations of the air inlet pipe tend to be stable, and the method of giving priority to the upper end of the air supply can promote the upward movement of the gas, so that the upper and lower adsorbent layers maintain a synchronous working state.

[0035] Optionally, the power assembly includes:

[0036] A rotating blade rotates in the air inlet pipe and rotates along with the supply of pressurized initial air;

[0037] The rotating shaft is connected with the rotating blades, rotates in the air intake pipe, and is connected with the rotating ring.

[0038] By adopting the above technical solution, the rotating blades are installed in the intake pipe and can rotate with the supplied pressurized initial gas (such as a mixture of ozone and oxygen); the rotating shaft is connected to the rotating blades and also rotates in the intake pipe, and the other end of the rotating shaft is connected to the rotating ring for transmitting the rotational torque; when the supply of pressurized initial gas begins, the gas enters the device through the intake pipe.

[0039] The power generated when the gas flows acts on the rotating blades, causing them to start rotating; as the rotating blades rotate, the rotating shaft also rotates; the rotating shaft transmits the rotational torque to the rotating ring through the connecting part, causing the rotating ring to start rotating; the rotation of the rotating ring causes the relative position with the sealing plate to change, and since the sealing plate is provided with a first protrusion, which abuts against the second protrusion on the rotating ring or other parts of the rotating ring, the rotation of the rotating ring will drive the sealing plate to move along the axial direction of the intake pipe or adjust its position; when the rotating ring rotates to a predetermined position, the sealing plate also reaches the target position; through the supply of pressurized initial gas, the rotation of the rotating blades is automatically realized, so that the rotating ring rotates automatically to adjust the position of the sealing plate; the power component uses the power generated by the supplied pressurized initial gas to drive the rotating blades to rotate, without the need for additional electricity or other energy; this reduces energy consumption and operating costs, while improving the self-driving and reliability of the system; by adjusting the flow and pressure of the supplied pressurized initial gas, the rotation speed of the rotating blades and the rotational torque of the rotating shaft can be controlled; this makes it possible to achieve precise adjustment of the sealing plate position to meet different work requirements.

[0040] At the same time, the rotating blades are set to hit the incoming pressurized initial gas, so that the internal gas components are mixed with each other, making the distribution of ozone more uniform, and giving ozone initial power, increasing the impact and contact with the adsorbent layer, making the adsorbent layer active, and improving the adsorption effect.

[0041] Optionally, the power assembly further includes:

[0042] A return spring is arranged in the air inlet pipe and connected to the sealing plate, and is used to push the sealing plate to approach the bottom of the tower body;

[0043] The limiting block is arranged in the air inlet pipe and abuts against an end of the sealing plate away from the rotating ring.

[0044] By adopting the above technical solution, in the initial state, the return spring is in a compressed or stretched state, exerting a thrust toward the bottom of the tower body on the sealing plate, and moving toward the bottom of the tower body in conjunction with the sealing plate's own gravity. The function of the limit block is to limit the maximum distance that the sealing plate can move upward to prevent it from moving excessively and damaging or affecting other components.

[0045] When the pressurized initial gas begins to be supplied, the gas enters the device through the air inlet pipe and acts on the rotating blades, causing them to start rotating; the rotation of the rotating blades is transmitted to the rotating ring through the rotating shaft, causing the rotating ring to start rotating; as the rotating ring rotates, the relative position between the sealing plate and the rotating ring changes, and driven by the rotating ring, the sealing plate begins to move along the axial direction of the air inlet pipe; at the same time, the return spring applies a continuous thrust to the sealing plate, so that it always maintains a movement trend toward the bottom of the tower body, but this thrust is overcome by the rotation of the rotating ring, allowing the sealing plate to move upward; when the rotating ring rotates to the predetermined position, the sealing plate also reaches the target position; at this time, the limit block abuts against the sealing plate to prevent it from continuing to move upward.

[0046] The introduction of the return spring enables the sealing plate to automatically return to its initial position after the supply of pressurized initial air is stopped. This feature improves the stability and reliability of the system and avoids failure or damage caused by improper position of the sealing plate. By adjusting the flow and pressure of the pressurized initial air supply, as well as the stiffness of the return spring and the position of the limit block, the movement distance and position of the sealing plate can be precisely controlled, which enables the system to meet different working requirements and achieve more precise control.

[0047] Optionally, the power assembly further includes:

[0048] A pressure pipe, one end of which is connected to a gas supply end for compressed initial gas;

[0049] The jet tube is provided with a plurality of other ends connected to the pressure tube, and the ends away from the pressure tube are connected to the air inlet pipe, and the ends away from the pressure tube are arranged along the axis of the rotating blade as the center of the circle and face the rotating blade.

[0050] By adopting the above technical scheme, one end of the pressure tube is connected to the air supply end of the pressurized initial gas to ensure a stable airflow supply. There are multiple jet tubes, one end of which is connected to the other end of the pressure tube to form a diversion. The ends of these jet tubes away from the pressure tube are evenly arranged with the axis of the rotating blade as the center, and their injection ports are facing the rotating blade; the rotating blade rotates freely in the intake pipe, and the return spring applies thrust to the sealing plate to keep it in the initial position, while the limit block limits the maximum distance the sealing plate moves upward; when the pressurized initial gas starts to be supplied, the gas first enters the jet tube through the pressure tube, and the jet tube sprays the gas onto the rotating blade at high speed. Since the injection ports are evenly arranged with the axis of the rotating blade as the center, the torque generated by the gas on the rotating blade is uniform, which helps the rotating blade to rotate smoothly.

[0051] This driving method does not require additional electricity or other energy, reducing energy consumption and operating costs; since the jet tubes are evenly arranged with the axis of the rotating blades as the center, the torque generated by the gas on the rotating blades is uniform, which helps the rotating blades to rotate smoothly and reduces vibration and noise; by adjusting the flow and pressure of the supplied pressurized initial gas, as well as the number and layout of the jet tubes, the rotation speed of the rotating blades and the rotational torque of the rotating shaft can be precisely controlled, which enables the system to meet different working requirements, achieve more precise control, and reduce the disorder of the pressurized initial gas and increase stability.

[0052] Optionally, the adsorbent layer comprises:

[0053] A partition frame is arranged at the upper end of the tower body to partition the upper end of the adsorption chamber into an operation chamber;

[0054] A first grid is slidably disposed in the tower body along the length direction of the tower body, is wavy in shape, and is slidably connected to the partition frame, and a first adsorbent layer is disposed on the grid;

[0055] A second grid is slidably disposed in the tower body along the length direction of the tower body and is in a wave shape. A second adsorbent layer is disposed on the second grid. The second adsorbent layer is correspondingly attached to the first adsorbent layer and can slide relative to the first adsorbent layer in the vertical direction.

[0056] The adjusting component is arranged on the partition frame, connected with the first grid frame and the second grid frame, and is used for driving the first grid frame or the second grid frame to slide.

[0057] By adopting the above technical solution, the partition frame is arranged at the upper end of the tower body, and the upper end of the reaction chamber is partitioned into an operating chamber, which is convenient for operations such as loading, unloading and replacing the adsorbent; the first grid and the second grid are both slidably arranged in the tower body along the length direction of the tower body, and both are wavy. This wavy design increases the surface area of ​​the adsorbent layer and improves the adsorption efficiency.

[0058] A first adsorbent layer is arranged on the first grid, and a second adsorbent layer is arranged on the second grid. The second adsorbent layer is correspondingly fitted to the first adsorbent layer, and the corresponding adsorption particles are staggered to form a stacked adsorption structure; an adjustment component is arranged on the partition frame and connected to the first grid and the second grid to control their sliding movement; during the adsorption process, the fixed first adsorption layer and the second adsorption layer are adsorbed, and the gas flushing position is adjusted through relative movement, so that the contact position of the gas changes, thereby realizing the combination of fixed adsorption and flow adsorption, increasing the contact area, and thus improving the adsorption efficiency.

[0059] And through the setting of the operating chamber, the first adsorbent layer and the second adsorbent layer can be replaced, and the particle size or number of layers of the adsorbent layer can be replaced. It is also possible to adjust the density inside the first frame and the second frame so that the first adsorbent layer and the second adsorbent layer float when sliding, thereby further improving the adsorption effect.

[0060] Optionally, the adjustment component includes:

[0061] A seesaw, rotatably disposed on the partition frame, one end of which is connected to the sealing plate and rotates with the sealing plate;

[0062] Two first lifting plates are provided, corresponding to the first grid frame and the second grid frame respectively, and a sliding groove is provided on one side of the first lifting plate located in the operation cavity, and the direction of the sliding groove is perpendicular to the sliding direction of the first grid frame;

[0063] The connecting shaft is arranged at one end of the seesaw plate away from the sealing plate, and slides and rotates in the sliding groove.

[0064] By adopting the above technical solution, during the sliding of the sealing plate, the seesaw is driven to rotate, the seesaw drives the first lifting plate to slide, the first lifting plate drives the first grid or the second grid to slide, or slide at different distances, to achieve relative movement between the two. Through the above arrangement, the automatic movement of the first grid or the second grid is achieved without the need for an additional power source, and the initial power of the pressurized initial gas is fully utilized for conversion to achieve effective and regular movement.

[0065] In summary, the present application includes at least one of the following beneficial technical effects:

[0066] 1. Adjusting the gas supply position to make the initial pressurized gas concentration in the ozone concentrator balanced can avoid the decrease in adsorption efficiency caused by local concentration being too high or too low, and ensure that the adsorbent can fully utilize its adsorption capacity; the combination of fixed adsorption and flow adsorption can dynamically adjust the use status of the adsorbent, avoiding the problem of too fast saturation or insufficient utilization of the adsorbent that may be caused by a single adsorption method, thereby improving the overall adsorption efficiency; using vacuum desorption can significantly reduce the pressure on the adsorbent surface, making it easier for the adsorbed ozone to desorb from the adsorbent, thereby improving the desorption efficiency and ozone recovery rate; the desorbed ozone can be further concentrated and purified after compression treatment, providing a high-quality, high-concentration ozone source for applications such as semiconductor material cleaning and etching;

[0067] 2. During the adsorption process, the fixed first adsorption layer and the second adsorption layer perform adsorption, and the gas flushing position is adjusted through relative movement, so that the contact position of the gas changes, and the fixed adsorption and flow adsorption are combined to increase the contact area and thus improve the adsorption efficiency;

[0068] 3. During the sliding of the sealing plate, the seesaw is driven to rotate, the seesaw drives the first lifting plate to slide, the first lifting plate drives the first grid or the second grid to slide, or slide at different distances to achieve relative movement between the two. Through the above settings, the automatic movement of the first grid or the second grid is achieved without the need for an additional power source, and the initial power of the pressurized initial gas is fully utilized for conversion to achieve effective and regular movement. BRIEF DESCRIPTION OF THE DRAWINGS

[0069] Figure 1 This is the overall structural diagram of the concentration device in the embodiment of the present application;

[0070] Figure 2 is a cross-sectional view of a tower body in an embodiment of the present application;

[0071] Figure 3 yes Figure 2 A magnified view of part A;

[0072] Figure 4 yes Figure 2 A magnified view of part B;

[0073] Figure 5 This is a structural diagram showing the adjustment component in the embodiment of the present application;

[0074] Figure 6 is an internal structure diagram of the first grid and the second grid in the embodiment of the present application;

[0075] Figure 7 This is a diagram showing the shapes of the first grid and the second grid in the embodiment of the present application.

[0076] Reference numerals: 100, tower body; 110, reaction chamber; 111, adsorption chamber; 112, impurity chamber; 113, operation chamber; 200, adsorbent layer; 210, partition frame; 220, first grid frame; 230, second grid frame; 240, first adsorbent layer; 250, second adsorbent layer; 260, adjustment component; 261, seesaw; 262, first lifting plate; 263, connecting shaft; 264, transmission rod; 265, transmission shaft; 266 , sliding groove; 267, force groove; 300, air inlet pipe; 310, air inlet hole; 400, exhaust pipe; 500, sealing plate; 510, connecting hole; 600, sliding mechanism; 610, rotating ring; 620, first protrusion; 630, second protrusion; 640, power assembly; 641, rotating blade; 642, rotating shaft; 643, return spring; 644, limit block; 645, pressure pipe; 646, jet pipe; 700, exhaust module. DETAILED DESCRIPTION

[0077] The following combination Figures 1 to 7 This application is described in further detail.

[0078] This embodiment discloses a high-purity ozone concentration process for cleaning and etching semiconductor materials.

[0079] The high-purity ozone concentration process used for cleaning and etching of semiconductor materials includes the following steps:

[0080] Gas compression: The mixed gas of ozone and oxygen is pressurized after dehydration to form a pressurized initial gas;

[0081] Specifically, ozone is prepared by using an ozone generator or other structures, or ozone gas is directly obtained by other means. The prepared ozone is doped with oxygen or other impurities, and most of the water is removed through a dehydration step, and then pressurized to further precipitate the water, and then proceed to the next step;

[0082] Adsorption separation: the pressurized initial gas is introduced into the ozone concentrator, and when it is introduced into the ozone concentrator, the pressurized initial gas is pumped and stirred, and the gas supply position of the pressurized initial gas is adjusted. When adjusting the gas supply position of the pressurized initial gas, the concentration of the pressurized initial gas inside the ozone concentrator is adjusted by intermittently supplying gas from bottom to top, so that the concentration of the pressurized initial gas in the ozone concentrator is balanced, and it contacts with the adsorbent in the ozone concentrator, and two layers of adsorbent are set to adsorb ozone together. During adsorption, an adjustment module is set to adjust the relative position of the two layers of adsorbent, change the flushing position of the gas, and form a combination of fixed adsorption and flow adsorption;

[0083] The adjustment module can adjust the position of the adsorbent by any linear sliding method;

[0084] Desorption: The ozone adsorbed by the adsorbent is separated from the adsorbent by vacuuming, and then compressed to form high-purity ozone concentrated gas.

[0085] The embodiment of the present application also discloses an ozone concentration device.

[0086] Reference Figure 1 and Figure 2The ozone concentration device comprises: a tower body 100 with a reaction chamber 110 formed therein, an adsorbent layer 200 arranged in the tower body 100 to divide the tower body 100 into an adsorption chamber 111 and a mixed gas chamber 112, an air inlet pipe 300 arranged on the tower body 100 for supplying air to the adsorption chamber 111, an exhaust pipe 400 arranged on the tower body 100 and connected to the mixed gas chamber 112 for exhaust, a sealing plate 500 slidably arranged on the air inlet pipe 300 for adjusting the communication between the air inlet pipe 300 and the adsorption chamber 111, a sliding mechanism 600 arranged on the air inlet pipe 300 for driving the sealing plate 500 to slide, and an exhaust module 700 arranged on the tower body 100 and connected to the adsorption chamber 111 for desorbing ozone; when ozone concentration is performed First, ozone is produced by an ozone generator or other ozone production equipment, and then the produced ozone gas is compressed to form a pressurized initial gas, and the pressurized initial gas is transported to the air inlet cavity through the air inlet pipe 300. During the transportation process, the sealing plate 500 is driven to slide by the sliding mechanism 600, so that the sealing plate 500 adjusts the gas entering the air inlet cavity from the air inlet pipe 300. The pressurized initial gas entering the air inlet cavity is adsorbed by the adsorbent layer 200, and the remaining gas enters the mixed gas cavity 112 and is then discharged through the exhaust pipe 400. After the adsorbent layer 200 is saturated with adsorption, the ozone adsorbed by the adsorbent layer 200 is desorbed by the exhaust module 700, and then compressed to form high-purity concentrated ozone.

[0087] The tower body 100 is cylindrical, and the reaction chamber 110 is opened in the vertical direction. The air inlet pipe 300 is cylindrical, and its axis coincides with the central axis of the reaction chamber 110. The air inlet pipe 300 extends from the bottom of the tower body 100 to the top of the tower body 100. A plurality of air inlet holes 310 are opened on the side wall of the air inlet pipe 300. The plurality of air inlet holes 310 are opened at equal intervals along the axial direction of the air inlet pipe 300, and the air inlet holes 310 are connected with the adsorption chamber 111; the processing module includes a negative pressure pipe, which is fixedly connected to the tower body 100, and is connected and communicated with one end of the negative pressure pipe close to the ground of the adsorption chamber 111. A switch valve is arranged on the negative pressure pipe, and a Roots vacuum pump is connected to the end of the negative pressure pipe away from the tower body 100, and a gas storage tank is connected to the air outlet end of the Roots vacuum pump; and valves are arranged on both the air inlet pipe 300 and the exhaust pipe 400 to facilitate the control of the switch of the gas passage.

[0088] The sealing plate 500 is sleeved inside the air inlet pipe 300 and fits with the inner wall of the air inlet pipe 300, and a sealing connection between the two can be achieved by a sealing ring. A plurality of connecting holes 510 are provided on the sealing plate 500, and the connecting holes 510 are correspondingly provided with the air inlet holes 310, and the opening length of the connecting holes 510 away from the tower body 100 along the length direction of the sealing plate 500 is greater than the length of the lower connecting holes 510, and the length difference is greater than or equal to the sliding distance of the sealing plate 500, and the lengths of the plurality of connecting holes 510 gradually increase along the direction approaching the top of the tower body 100, the connecting holes 510 near the bottom wall of the tower body 100 and the corresponding air inlet holes 310 are completely staggered and closed, the connecting holes 510 near the top of the tower body 100 and the corresponding air inlet holes 310 are completely connected, and as the sealing plate 500 moves upward, the connecting holes 510 near the bottom wall and the corresponding air inlet holes 310 are completely connected, and the connecting holes 510 near the top are always connected with the corresponding air inlet holes 310.

[0089] Reference Figure 2 and Figure 3 The sliding mechanism 600 includes a rotating ring 610 rotatably connected to the air inlet pipe 300. The rotating ring 610 is located at one end of the sealing plate 500 close to the bottom of the tower body 100. The rotating ring 610 is coaxial with the air inlet pipe 300. A first protrusion 620 is fixedly connected to the rotating ring 610. A plurality of first protrusions 620 may be provided. In this embodiment, two are preferably provided, and both are located on the side of the rotating ring 610 close to the sealing plate 500. The cross-sectional area of ​​the end of the first protrusion 620 away from the rotating ring 610 is smaller than the cross-sectional area of ​​the end close to the rotating ring 610. The cross-sectional area may be triangular, trapezoidal or other shapes, and the tip abuts against the end face of the sealing plate 500. A second protrusion 630 is fixedly connected to one side of the plate 500 close to the rotating ring 610. The second protrusion 630 corresponds to the first protrusion 620 and has a similar structure. The second protrusion 630 and the first protrusion 620 are alternately arranged, and the second protrusion 630 can abut against the rotating ring 610; as the rotating ring 610 rotates, the ends of the first protrusion 620 and the second protrusion 630 can be driven to abut against each other, so that the sealing plate 500 slides, thereby adjusting the relative positions of the connecting hole 510 and the air inlet hole 310; a power assembly 640 is arranged in the air inlet pipe 300, and the power assembly 640 is connected to the rotating ring 610, so as to drive the rotating ring 610 to rotate.

[0090] The power assembly 640 includes a rotating blade 641 rotatably connected to the inner wall of the intake pipe 300, and a rotating shaft 642 is coaxially fixedly connected to the rotating blade 641. The rotating shaft 642 is coaxially arranged with the intake pipe 300 and coaxially fixedly connected with the rotating ring 610. The rotating blade 641 is rotated by blowing the pressurized initial air, thereby driving the rotating ring 610 to rotate, thereby realizing the relative position change of the first protrusion 620 and the second protrusion 630.

[0091] Reference Figure 2 and Figure 4 In order to facilitate the free reset of the sealing plate 500, a mounting groove is opened on the inner wall of the air inlet pipe 300, and a reset spring 643 is fixedly connected in the mounting groove. The reset spring 643 is located between the sealing plate 500 and the air inlet pipe 300, and is connected to the sealing plate 500, and is used to drive the sealing plate 500 to approach the bottom of the tower body 100.

[0092] Reference Figure 5 In order to reduce excessive sliding of the sealing plate 500 during the sliding process, a limit block 644 is fixedly connected inside the air intake pipe 300. The limit block 644 is located at one end of the sealing plate 500 away from the rotating ring 610 and abuts against the sealing plate 500 to limit excessive sliding of the sealing plate 500.

[0093] In order to reduce the instability of the pressurized initial gas, the power assembly 640 also includes a pressure tube 645, which is fixedly connected to the tower body 100 and extends into the tower body 100. One end extending into the tower body 100 is fixedly connected to a plurality of jet tubes 646. The jet tubes 646 are closely arranged along the circumference of the pressure tube 645 and connected to the pressure tube 645. One end of the jet tube 646 away from the pressure tube 645 is connected to the air intake pipe 300, and is evenly arranged along the axis of the rotating blade 641 as the center of the circle. The jet tube 646 is inclined toward the rotating blade 641.

[0094] Reference Figures 5 to 7 The adsorbent layer 200 includes a partition frame 210 fixedly connected to the inner wall of the tower body 100, the partition frame 210 partitions the upper end of the reaction chamber 110 into an operation chamber 113, and the operation chamber 113 is not connected to the adsorption chamber 111 and the impurity chamber 112; the partition frame 210 is slidably connected with a first grid frame 220 and a second grid frame 230, the first grid frame 220 and the second grid frame 230 are both wavy ring-shaped, and the second grid frame 230 is smaller than the first grid frame 220, the second grid frame 230 is in contact with the first grid frame 220 and the wave position corresponds, and the first grid frame 220 and the second grid frame 230 can slide relatively; the first grid frame 220 is in contact with the first grid frame 220. A first installation bin is formed, and the first installation bin is filled with a first adsorbent layer 240; a second installation bin is formed in the second grid 230, and the second installation bin is filled with a second adsorbent layer 250. The wall thickness of the first installation bin and the second installation bin is very small, so that the first adsorbent layer 240 and the second adsorbent layer 250 can be in contact with each other, and the adsorbent particles of the first adsorbent layer 240 and the second adsorbent layer 250 are staggered or supplemented; an adjustment component 260 is arranged on the partition frame 210, and the adjustment component 260 is connected to the first grid 220 and the second grid 230, and is used to drive the first grid 220 and the second grid 230 to slide.

[0095] The adjustment component 260 can adopt any mechanical structure that can achieve linear displacement, such as a cylinder, a motor rack, an electromagnetic linear displacement servo regulator, etc.; the present embodiment is preferably of the following structure, the adjustment component 260 includes a plurality of transmission rods 264 fixedly connected to the sealing plate 500, the transmission rod 264 is slidably connected to the partition frame 210, and extends into the operating chamber 113; the partition frame 210 is rotatably connected to a side wall away from the air intake pipe 300, and a plurality of seesaws 261 are rotatably connected, the seesaws 261 are evenly spaced along the circumference of the air intake pipe 300, and the end of the seesaw 261 with a shorter force arm is close to the transmission rod 264; a force application groove 267 is provided at the end of the seesaw 261 close to the transmission rod 264, and the force application groove 267 is provided along the length direction of the seesaw 261, and a transmission shaft 265 is fixedly connected to the transmission rod 264, and the transmission shaft 265 partially rotates and slides. In the force-applying groove 267, during the upward movement of the transmission rod 264, the seesaw 261 is driven to rotate through the transmission shaft 265 and the force-applying groove 267; the first lifting plate 262 is fixedly connected to the first grid 220 and the second grid 230, and the first lifting plate 262 is L-shaped, and the two first lifting plates 262 are arranged back to back. A sliding groove 266 is opened at one end of the first lifting plate 262 away from the first grid 220, and the opening direction of the sliding groove 266 is parallel to the radial direction of the water inlet pipe. In the sliding groove 266, a connecting shaft 263 is slidingly and rotatably connected, and the connecting shaft 263 is fixedly connected to one end of the seesaw 261 away from the transmission rod 264. As the seesaw 261 rotates, with the cooperation of the connecting shaft 263 and the sliding groove 266, the first grid 220 and the second grid 230 move up at different amplitudes, thereby generating relative displacement.

[0096] In other embodiments, the installation of the adsorbent in the first installation bin and the second installation bin can be reduced, so that the adsorbent is in a slightly active state, the activity space is one-fifth of the particle size, and the multiple layers are staggered. When the first frame 220 and the second frame 230 slide, the adsorbent can be in a suspended state to form a fluidized bed, thereby optimizing the adsorption efficiency.

[0097] In other embodiments, multiple concentrating devices may be provided to perform cyclic operation.

[0098] The implementation principle of an ozone concentration device in an embodiment of the present application is as follows: when performing ozone concentration work, firstly, an ozone mixed gas is obtained through existing equipment, and then a pressurized initial gas is formed through a dehydration and pressurization step, and then the pressurized initial gas is passed into a pressure tube 645, and the pressurized initial gas passes through the pressure tube 645 and enters the jet tube 646. The pressurized initial gas in the jet tube 646 blows the rotating blade 641, and the rotating blade 641 drives the rotating ring 610 to rotate through the rotating shaft 642, and the rotating ring 610 drives the second protrusion 630 to rotate. Through friction with the second protrusion 630, and the cooperation of the return spring 643 and the limit block 644, the sealing plate 500 slides back and forth in the vertical direction, so that the lower end air inlet 310 is reciprocally connected or closed with the air inlet cavity. After the pressurized initial gas enters the adsorption chamber 111, the ozone is adsorbed by the adsorbent, and the remaining gas is discharged through the mixed gas cavity 112 and the exhaust pipe 400.

[0099] During the sliding of the sealing plate 500, the sealing plate 500 drives the transmission rod 264 to slide back and forth, the transmission rod 264 drives the seesaw 261 to rotate through the transmission shaft 265, and the seesaw 261 drives the first lifting plate 262 to slide through the connecting shaft 263, so that the first grid 220 and the second grid 230 slide. The sliding distances of the first grid 220 and the second grid 230 are different, resulting in misalignment, which increases the contact area between the adsorbent and ozone, thereby improving the adsorption effect.

[0100] After the ozone adsorption is completed or the adsorbent is saturated, the exhaust pipe 400 is blocked and connected to the exhaust module 700. The ozone adsorbed by the adsorbent is discharged by vacuuming and concentrated and stored.

[0101] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A high-purity ozone concentration device used for cleaning and etching of semiconductor materials, characterized in that: include: The tower body (100) has a reaction chamber (110) formed therein; An adsorbent layer (200) is arranged in the tower body (100), is arranged in a ring shape around the central axis of the tower body (100), and divides the reaction chamber (110) into an adsorption chamber (111) and a mixed gas chamber (112); an air inlet pipe (300) disposed on the tower body (100), extending from the bottom to the top of the tower body (100), and located in the adsorption chamber (111), and having a plurality of air inlet holes (310) in communication with the adsorption chamber (111); An exhaust pipe (400) is disposed on the tower body (100) and is in communication with the impurity chamber (112) and is used to exhaust the remaining gas after adsorption is completed; A sealing plate (500) is slidably mounted in the air inlet pipe (300) and is provided with a plurality of communication holes (510) in a vertical direction. The communication holes (510) correspond to and are connected to the air inlet holes (310). In an initial state, the air inlet holes (310) at the lower end are offset and blocked from the communication holes (510). As the sealing plate (500) slides, the air inlet holes (310) at the lower end are opened. A sliding mechanism (600) is arranged on the air inlet pipe (300), connected to the sealing plate (500), and used to drive the sealing plate (500) to slide; An exhaust module (700) is communicated with the adsorption chamber (111) and is used to extract the ozone adsorbed by the adsorbent layer (200) for compression; The sliding mechanism (600) comprises: A rotating ring (610) is rotatably disposed in the air inlet pipe (300) and abuts against an end of the sealing plate (500) close to the bottom wall of the tower body (100); A first protrusion (620) is provided on the rotating ring (610), faces the sealing plate (500), and abuts against the sealing plate (500); A second protrusion (630) is provided on the sealing plate (500) and abuts against the first protrusion (620) or the rotating ring (610); A power assembly (640) is disposed in the air intake pipe (300), connected to the rotating ring (610), and used to drive the rotating ring (610) to rotate; The adsorbent layer (200) comprises: A partition frame (210) is arranged at the upper end of the tower body (100) and partitions the upper end of the adsorption chamber (111) into an operation chamber (113); A first grid (220) is slidably disposed in the tower body (100) along the length direction of the tower body (100), is wavy in shape, is slidably connected to the partition frame (210), and has a first adsorbent layer (240) disposed thereon; A second grid (230) is slidably disposed in the tower body (100) along the length direction of the tower body (100) and is in a wave shape, on which a second adsorbent layer (250) is disposed, the second adsorbent layer (250) being correspondingly fitted to the first adsorbent layer (240) and capable of relative sliding in a vertical direction; an adjustment component (260), arranged on the partition frame (210), connected to the first grid frame (220) and the second grid frame (230), and used for driving the first grid frame (220) or the second grid frame (230) to slide; The adjustment component (260) comprises: A seesaw (261) is rotatably disposed on the partition frame (210), one end of which is connected to the sealing plate (500) and rotates along with the sealing plate (500); Two first lifting plates (262) are provided, corresponding to the first grid frame (220) and the second grid frame (230) respectively, and a sliding groove (266) is provided on one side of the first lifting plate (262) located in the operating cavity (113), and the opening direction of the sliding groove (266) is perpendicular to the sliding direction of the first grid frame (220); The connecting shaft (263) is arranged at one end of the seesaw (261) away from the sealing plate (500), and slides and rotates in the sliding groove (266).

2. The high-purity ozone concentration device for cleaning and etching semiconductor materials according to claim 1 is characterized in that: The power assembly (640) comprises: A rotating blade (641) rotates in the air inlet pipe (300) and rotates as the pressurized initial air is supplied; The rotating shaft (642) is connected to the rotating blade (641), rotates in the air intake pipe (300), and is connected to the rotating ring (610).

3. The high-purity ozone concentration device for cleaning and etching semiconductor materials according to claim 2 is characterized in that: The power assembly (640) further includes: A return spring (643) is disposed in the air inlet pipe (300), connected to the sealing plate (500), and used to push the sealing plate (500) close to the bottom of the tower body (100); A limit block (644) is disposed in the air inlet pipe (300) and abuts against an end of the sealing plate (500) away from the rotating ring (610).

4. The high-purity ozone concentration device for cleaning and etching semiconductor materials according to claim 2 or 3, characterized in that: The power assembly (640) further includes: A pressure pipe (645) having one end connected to a gas supply end for compressed initial gas; The jet tube (646) is provided with a plurality of other ends connected to the pressure tube (645), and the ends away from the pressure tube (645) are all connected to the air intake pipe (300), and the ends away from the pressure tube (645) are all arranged along the axis of the rotating blade (641) as the center of the circle and face the rotating blade (641).

5. An ozone concentration process using the high-purity ozone concentration device for cleaning and etching semiconductor materials as described in any one of claims 1 to 4, characterized in that: The following steps are involved: Gas compression: The mixed gas of ozone and oxygen is pressurized after dehydration to form a pressurized initial gas; Adsorption separation: the pressurized initial gas is introduced into the ozone concentrator, and when the pressurized initial gas is introduced into the ozone concentrator, the gas supply position of the pressurized initial gas is adjusted so that the concentration of the pressurized initial gas in the ozone concentrator is balanced and in contact with the adsorbent in the ozone concentrator; two layers of adsorbent are set to jointly adsorb ozone, and the adsorbents in the two adsorbent layers are in an active state, and during adsorption, the adsorbent layers are in a suspended state to form a fluidized bed; an adjustment module is set to adjust the relative positions of the two adsorbent layers, so that the two adsorbent layers are relatively displaced, the flushing position of the gas is changed, and a combination of fixed adsorption and flow adsorption is formed; Desorption: The ozone adsorbed by the adsorbent is separated from the adsorbent by vacuuming, and then compressed to form high-purity ozone concentrated gas; In the adsorption separation step, when the pressurized initial gas is supplied, the pressurized initial gas is pumped and agitated.

6. The ozone concentration process according to claim 5, characterized in that: In the adsorption separation step, when adjusting the supply position of the pressurized initial gas, an intermittent gas supply from bottom to top is adopted to adjust the concentration of the pressurized initial gas inside the ozone concentrator.

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